Table of Contents

Locator Record

Title: Urinary Organophosphate Insecticides: Diakyl Phosphate Metabolites (L26OPD_C )
Contact Number: 1-866-441-NCHS
Years of Content: 2003 - 2004
First Published: June, 2009
Revised: NA
Access Constraints: None
Use Constraints: None
Geographic Coverage: National
Subject:Urinary Organophosphate Insecticides: Diakyl Phosphate Metabolites
Record Source: NHANES 2003 - 2004
Survey Methodology: NHANES 2003 - 2004 is a stratified multistage probability sample of the civilian non-institutionalized population of the U.S.
Medium: NHANES Web site; SAS transport files

Component Description

Organophosphorus insecticides, which are active against a broad spectrum of insects, have accounted for a large share of all insecticides used in the United States. Although organophosphorus insecticides are still used for insect control on many food crops, most residential uses have been phased out in the United States as a result of implementation of the Food Quality Protection Act of 1996. Pesticide residues and their metabolites in human tissues and fluids can be indicative of pesticide exposure and the total body burden of these pesticides. About 75% of registered organophosphorus insecticides are metabolized in the body to measurable dialkyl phosphate (DAP) metabolites. Dialkyl phosphates may also occur in the environment as a result of degradation of organophosphorus insecticides, and therefore, the presence in a person’s urine may reflect exposure to the metabolite itself.

Generally, six urinary dialkyl phosphate metabolites of organophosphorus insecticides have been measured: dimethylphosphate (DMP); dimethylthiophosphate (DMTP); dimethyldithiophosphate (DMDTP); diethylphosphate (DEP); diethylthiophosphate (DETP); and diethyldithiophosphate (DEDTP). Each of the six urinary dialkyl phosphate metabolites can be produced from the metabolism of more than one organophosphorus insecticide or may be present following ingestion of the specific DAP metabolite. Therefore, the presence of one or more dialkyl phosphate metabolites without additional information cannot be linked to exposure to a specific organophosphorus insecticide.

Eligible Sample

Participants aged 6 years and older who met the subsample requirements.

Description of Laboratory Methodology

This method was developed for quantifying the six DAP urinary metabolites of at least 28 organophosphorus pesticides using lyophilization and chemical derivatization followed by analysis using isotope-dilution gas chromatography–tandem mass spectrometry (GC–MS/MS). Urine samples were spiked with stable isotope analogues of the DAPs and the water was removed from the samples using a lyophilizer. The dried residue was dissolved in acetonitrile and diethyl ether, and the DAPs were chemically derivatized to their respective chloropropyl phosphate esters. The chloropropyl phosphate esters were concentrated, and analyzed using GC–MS/MS. The limits of detection of the method were in the low mg/l (parts per billion) to mid pg/ml range (parts per trillion) with coefficients of variation of 7–14%. The use of stable isotope analogues as internal standards for each of these metabolites allows for sample-specific adjustment for recovery and thus permits a high degree of accuracy and precision. Use of this method with approximately 1100 urine samples collected from pregnant women and children indicate that the low limits of detection allow this method to be used in general population studies.

Laboratory Quality Assurance and Monitoring

Urine specimens are processed, stored, and shipped to the Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention for analysis.
Detailed specimen collection and processing instructions are discussed in the NHANES Laboratory/Medical Technologists Procedures Manual (LPM). Vials are stored under appropriate frozen (–20°C) conditions until they are shipped to National Center for Environmental Health for testing.

Mobile Examination Centers (MECs)

Laboratory team performance is monitored using several techniques. NCHS and contract consultants use a structured quality assurance evaluation during unscheduled visits to evaluate both the quality of the laboratory work and the quality-control procedures. Each laboratory staff person is observed for equipment operation, specimen collection and preparation; testing procedures and constructive feedback are given to each staff. Formal retraining sessions are conducted annually to ensure that required skill levels were maintained.

The NHANES QA/QC protocols meet the 1988 Clinical Laboratory Improvement Act mandates. Detailed QA/QC instructions are discussed in the NHANES LPM.

Analytical Laboratories

NHANES uses several methods to monitor the quality of the analyses performed by the laboratories. In the MEC, these methods include performing blind split samples collected on “dry run” sessions. In addition, contract laboratories randomly perform repeat testing on 2.0% of all specimens.

NCEH developed and distributed a quality control protocol for all the laboratories which outlined the Westgard rules used when running NHANES specimens. Any problems encountered during shipping or receipt of specimens, instrument calibration, reagents, and any special considerations are submitted to NCHS and Westat. Summary statistics for each control pool, QC graphs, are reviewed by NCHS for trends or shifts in the data. The laboratories are required to explain any identified areas of concern.

All QC procedures recommended by the manufacturers were followed. Reported results for all assays meet the Division of Laboratory Sciences’ quality control and quality assurance performance criteria for accuracy and precision (similar to specifications outlined by Westgard (1981).

Analytic Notes

Subsample weights

Measures of urinary diakyl phosphate metabolites were measured in a one third subsample of persons 6 years and over. Special sample weights are required to analyze these data properly. Specific sample weights for this subsample are included in this data file and should be used when analyzing these data.

Variance estimation

The analysis of NHANES 2003-2004 laboratory data must be conducted with the key survey design and basic demographic variables. The NHANES 2003-2004 Demographic Data File contains demographic and sample design variables. The recommended procedure for variance estimation requires use of stratum and PSU variables (SDMVSTRA and SDMVPSU, respectively) in the demographic data file.

Links to NHANES Data Files

This laboratory data file can be linked to the other NHANES 2003-2004 data files using the unique survey participant identifier SEQN.

Detection Limits

The detection limits were constant for all of the analytes except for diethyldithiophosphate (URXOP6) in the data set. Diethyldithiophosphate (URXOP6) has two detection limits. Two variables are provided for each of these analytes. The variable named URD___LC indicates whether the result was below the limit of detection. There are two values: “0” and “1”. “0” means that the result was at or above the limit of detection. “1” indicates that the result was below the limit of detection.

The other variable named URX___ provides the analytic result for that analyte.

The detection limit divided by the square root of 2 is the value that is provided for results that are below the limit of detection.

The lower limit of detections for the diakyl phosphate metabolites is:

Lower Limit of Detections for the Diakyl Phosphate Metabolites
Analyte Item ID  Limit of Detection (LLOD)
Dimethylphosphate URXOP1 0.5
Diethylphosphate URXOP2 0.1
Dimethylthiophosphate URXOP3 0.5
Diethylthiophosphate URXOP4 0.2
Dimethyldithiophosphate URXOP5 0.1
Diethyldithiophosphate URXOP6 0.1

Please refer to the Analytic Guidelines for further details on the use of sample weights and other analytic issues.

References

Codebook and Frequencies

SEQN - Respondent sequence number

Variable Name:
SEQN
SAS Label:
Respondent sequence number
English Text:
Respondent sequence number
Target:
Both males and females 6 YEARS - 150 YEARS

WTSC2YR - Two-year MEC weights of subsample C

Variable Name:
WTSC2YR
SAS Label:
Two-year MEC weights of subsample C
English Text:
Two-year MEC weights of subsample C
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
0 to 456851.11941 Range of Values 2612 2612
. Missing 0 2612

URXOP1 - Dimethylphosphate (ug/L)

Variable Name:
URXOP1
SAS Label:
Dimethylphosphate (ug/L)
English Text:
Dimethylphosphate (ug/L)
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
0.35 to 133.62 Range of Values 2494 2494
. Missing 118 2612

URDOP1LC - Dimethylphosphate comment code

Variable Name:
URDOP1LC
SAS Label:
Dimethylphosphate comment code
English Text:
Dimethylphosphate comment code
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
0 At or above the detection limit 1234 1234
1 Below lower detection limit 1260 2494
. Missing 118 2612

URXOP2 - Diethylphosphate (ug/L)

Variable Name:
URXOP2
SAS Label:
Diethylphosphate (ug/L)
English Text:
Diethylphosphate (ug/L)
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
0.07 to 4481.79 Range of Values 2453 2453
. Missing 159 2612

URDOP2LC - Diethylphosphate comment code

Variable Name:
URDOP2LC
SAS Label:
Diethylphosphate comment code
English Text:
Diethylphosphate comment code
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
0 At or above the detection limit 1255 1255
1 Below lower detection limit 1198 2453
. Missing 159 2612

URXOP3 - Dimethylthiophosphate (ug/L)

Variable Name:
URXOP3
SAS Label:
Dimethylthiophosphate (ug/L)
English Text:
Dimethylthiophosphate (ug/L)
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
0.35 to 1058.04 Range of Values 2494 2494
. Missing 118 2612

URDOP3LC - Dimethylthiophosphate comment code

Variable Name:
URDOP3LC
SAS Label:
Dimethylthiophosphate comment code
English Text:
Dimethylthiophosphate comment code
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
0 At or above the detection limit 1961 1961
1 Below lower detection limit 533 2494
. Missing 118 2612

URXOP4 - Diethylthiophosphate (ug/L)

Variable Name:
URXOP4
SAS Label:
Diethylthiophosphate (ug/L)
English Text:
Diethylthiophosphate (ug/L)
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
0.14 to 83.15 Range of Values 2422 2422
. Missing 190 2612

URDOP4LC - Diethylthiophosphate comment code

Variable Name:
URDOP4LC
SAS Label:
Diethylthiophosphate comment code
English Text:
Diethylthiophosphate comment code
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
0 At or above the detection limit 1289 1289
1 Below lower detection limit 1133 2422
. Missing 190 2612

URXOP5 - Dimethyldithiophosphate (ug/L)

Variable Name:
URXOP5
SAS Label:
Dimethyldithiophosphate (ug/L)
English Text:
Dimethyldithiophosphate (ug/L)
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
0.07 to 80.51 Range of Values 2458 2458
. Missing 154 2612

URDOP5LC - Dimethyldithiophosphate comment code

Variable Name:
URDOP5LC
SAS Label:
Dimethyldithiophosphate comment code
English Text:
Dimethyldithiophosphate comment code
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
0 At or above the detection limit 997 997
1 Below lower detection limit 1461 2458
. Missing 154 2612

URXOP6 - Diethyldithiophosphate (ug/L)

Variable Name:
URXOP6
SAS Label:
Diethyldithiophosphate (ug/L)
English Text:
Diethyldithiophosphate (ug/L)
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
0.07 to 12.67 Range of Values 2494 2494
. Missing 118 2612

URDOP6LC - Diethyldithiophosphate comment code

Variable Name:
URDOP6LC
SAS Label:
Diethyldithiophosphate comment code
English Text:
Diethyldithiophosphate comment code
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
0 At or above the detection limit 224 224
1 Below lower detection limit 2270 2494
. Missing 118 2612

URXUCR - Creatinine, urine (mg/dL)

Variable Name:
URXUCR
SAS Label:
Creatinine, urine (mg/dL)
English Text:
Creatinine, urine (mg/dL)
Target:
Both males and females 6 YEARS - 150 YEARS
Code or Value Value Description Count Cumulative Skip to Item
7 to 648 Range of Values 2530 2530
. Missing 82 2612